Sodium Phosphate, Dibasic → HCID 15612026, compound

HRID 1199294Notes

Reaction equation

HRID 1199294 reaction equation
[Mn]([O-])(=O)(=O)=O.[K+].P([O-])([O-])(O)=[O:8].[Na+].[Na+].[Cl:14][C:15]1[C:16]([O:23][C:24]2[N:29]=[C:28]([O:30][CH3:31])[CH:27]=[C:26]([O:32][CH3:33])[N:25]=2)=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:18]=[O:19]>CC(C)=O>[Cl:14][C:15]1[C:16]([O:23][C:24]2[N:25]=[C:26]([O:32][CH3:33])[CH:27]=[C:28]([O:30][CH3:31])[N:29]=2)=[C:17]([CH:20]=[CH:21][CH:22]=1)[C:18]([OH:8])=[O:19]

Participants

5

Procedure

An aqueous solution of potassium permanganate (1.3 g) and disodium hydrogenphosphate (1 g) was dropwise added to a solution of 3-chloro-2-(4,6-dimethoxypyrimidin-2-yl)oxy benzaldehyde (1.7 g) in acetone (50 ml). The mixture was stirred at room temperature for 12 hours, and the precipitated manganese dioxide was filtered off. The filtrate was adjusted with hydrochloric acid to a pH of about 4 and then extracted with chloroform. The chloroform layer was washed with water and dried, and the solvent was distilled off under reduced pressure. The residue thus obtained was recrystallized from carbon tetrachloride to obtain the above identified compound as a white solid (1.1 g). (Melting point: 151°-152° C.).

Workup

  1. filtrationthe precipitated manganese dioxide was filtered off
  2. extractionextracted with chloroform
  3. washThe chloroform layer was washed with water
  4. customdried
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue thus obtained
  7. customwas recrystallized from carbon tetrachloride
  8. customto obtain the

Sources & evidence

ORD record
ord-158a3e3b57c74c47abe4b5e818e1b948
Source dataset
uspto-grants-1990_02
Patent number
US04900352

Reaction notes

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